CN103074553A - Fe-Cr-Si ternary amorphous thin film capable of modulating band gap width and preparation method thereof - Google Patents

Fe-Cr-Si ternary amorphous thin film capable of modulating band gap width and preparation method thereof Download PDF

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CN103074553A
CN103074553A CN2013100166021A CN201310016602A CN103074553A CN 103074553 A CN103074553 A CN 103074553A CN 2013100166021 A CN2013100166021 A CN 2013100166021A CN 201310016602 A CN201310016602 A CN 201310016602A CN 103074553 A CN103074553 A CN 103074553A
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CN103074553B (en
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李晓娜
郑月红
董闯
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Dalian University of Technology
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Abstract

The invention discloses a Fe-Cr-Si ternary amorphous thin film capable of modulating band gap width and a preparation method thereof, and belongs to the technical field of semiconductor materials. The Fe-Cr-Si ternary amorphous thin film has the following general formula: Fe3Cr1Six, wherein x is 8-18; along with increase of x from 8 to 18, the band gap width increases from 0 eV to 0.65 eV; and the thin film structure is amorphous. Compared with an ordinary binary transition metal silicide thin film, the Fe-Cr-Si ternary amorphous thin film has the advantages as follows: 1, the Fe3Cr1Six thin film is a novel ternary semiconductor amorphous thin film and can modulate the band gap width within a relatively large range of 0-0.65 eV; and under the action of Cr, the band gap width can be affected and the amorphous forming capability of the thin film can be increased through addition of one element; 2, the proportion of Si in the Fe3Cr1Six thin film can be conveniently regulated only by changing the number of Fe3Cr1 alloys in a combined sputtering target, thus obtaining different band gap widths; and 3, the Fe3Cr1Six thin film is amorphous, so that the uniformity of components and the performance can be ensured, and lattice mismatch and multiphase mixing and other problems during preparation of a crystalline thin film are effectively avoided. Therefore, the Fe-Cr-Si ternary amorphous thin film is applicable to production of near infrared detectors and other semiconductor devices with narrow band gaps.

Description

A kind of Fe-Cr-Si that modulates band gap width is ternary noncrystal membrane and preparation method thereof
Technical field
The present invention relates to a kind of Fe-Cr-Si ternary noncrystal membrane of modulating band gap width and preparation method thereof, belong to technical field of semiconductor.
Background technology
Semiconductor metallic silicides is one of used for solar batteries material, they and single silicon have fabulous consistency, have the electroconductibility of metal, high thermostability, oxidation-resistance and superior mechanical stability, the semiconductor silicon compound has also won widely with its superior environmental friendliness characteristic and has paid close attention to simultaneously, especially transition metal-silicon.β-FeSi is wherein typically arranged 2And CrSi 2β-FeSi 2Have 0.83 ~ 0.87eV direct band gap, to infrared wavelength have larger photoabsorption coefficient (α〉10 -5Cm -1, 1.0eV), the theoretical light photoelectric transformation efficiency can reach 16 ~ 23%, can be used for preparing efficient solar cell, photodiode, photo-detector etc.It has potential using value equally in thermoelectric field simultaneously, can be used for preparing thermal generator, thermal sensor etc.CrSi 2Also be a kind of P-type semiconductor, its have narrower band gap (0.30 ~ 0.35eV), compare CrSi with other transition metal semi-conductor silicide material 2Has minimum lattice mismatch rate between crystal and the silicon substrate.
Current preparation β-FeSi 2The problem that exists is as follows:
(1) β-FeSi 2Be a kind of ol cpds, when preparation body material or thin-film material, all very easily generate other intermediate compound of Fe and Si (such as ε-FeSi and α-FeSi 2), the heterogeneous situation that mixes appears.Also very easily occur the defectives such as fault, twin in its crystal, therefore be difficult to obtain the pure β-FeSi of high quality 2Material.
(2) β-FeSi 2When being used for photoelectric field, most take single crystalline Si as base preparation film, but have larger film base mismatch problems, cause its a lot of performances to fail to reach theory expectation.
(3) use at present the binary β of different methods preparation-FeSi 2Material, its band gap width changes about 0.87eV, though slightly different, can not modulate.Add the crystalline state ternary FeSi behind the 3rd constituent element 2Shaped material then is easy to the phenomenon that occurs being separated, although band gap width can be modulated in a big way, has increased the unstable of structure, so that the heterogeneous situation that mixes further worsens.
Summary of the invention
The present invention is directed to above-mentioned deficiency, at binary β-FeSi 2On the basis of research, with Cr element substitution β-FeSi 2A Fe element of/4th in the structure comes in a big way modulation band gap width by the content of adjusting Si in the Fe-Cr-Si three-part system.Adopt simultaneously the mode of preparation noncrystalline membrane, effectively avoid in the crystalline film lattice mismatch and the heterogeneous problem such as mix, and non-crystalline state can guarantee homogeneous chemical composition, and then guaranteed performance is stable.The present invention is intended to prepare a kind of Fe-Cr-Si ternary noncrystal membrane of modulating band gap width, thereby improves the use properties of material, the scope of application of expansion material.
The technical solution used in the present invention is: a kind of Fe-Cr-Si that modulates band gap width is that the ternary noncrystal membrane has following general formula: Fe 3Cr 1Si x, x is 8 ~ 18; Along with x is increased to 18 from 8, the band gap width of this Amorphous Films is increased to 0.65eV from 0, and membrane structure is always non-crystalline state.
The preparation method that the described Fe-Si-Cr that modulates band gap width is the ternary noncrystal membrane adopts the following step:
(1) preparation alloy sputtering target, its step is as follows:
1. get the raw materials ready: take by weighing each constituent element value according to Fe and Cr atomic percent 3:1, the purity of stand-by Fe, Cr raw metal is more than 99. 9%;
2. Fe 3Cr 1The melting of alloy pig: the compound of metal is placed in the water jacketed copper crucible of smelting furnace, adopts the method for vacuum arc melting under the protection of argon gas, to carry out melting, at first be evacuated to 10 -2Pa, then being filled with argon gas to air pressure is 0.03 ± 0.01MPa, the span of control of melting current density is 150 ± 10A/cm 2, after the fusing, continuing again 10 seconds of melting, outage allows alloy be cooled to room temperature with copper crucible, then with its upset, again places in the water jacketed copper crucible, carries out the melting second time; Aforementioned process melt back at least 3 times obtains the Fe of homogeneous chemical composition 3Cr 1Alloy pig;
3. Fe 3Cr 1The preparation of alloy bar: with Fe 3Cr 1Alloy pig places in the water jacketed copper crucible that is connected with negative pressure suction casting equipment, with above-mentioned vacuum arc melting method molten alloy, at first is evacuated to 10 under argon shield -2Pa, then being filled with argon gas to air pressure is 0.03 ± 0.01MPa, the used current density of melting is 150 ± 10A/cm 2, after the fusing, continuing again 10 seconds of melting, the negative pressure absorbing and casting device is opened in outage simultaneously, allows alloy melt be filled with in the cylindrical, copper model cavity, is cooled to room temperature, obtains requiring the Fe of specification 3Cr 1Alloy bar;
4. the preparation of alloy paster: the alloy small pieces that alloy bar are cut into desired thickness with the low speed saw;
5. the preparation of alloy sputtering target: with conductive silver glue with Fe 3Cr 1It is on 99.999% the basic Si target, perhaps with Fe that alloy slice sticks on the used purity of sputter 3Cr 1It is to make the combined alloy sputtering target material on the 99.999% basic Si target that alloy slice directly is mounted to porose purity;
(2) preparation Fe-Si-Cr is the ternary noncrystal membrane, and its step is as follows:
1. Si (100) and the Al of Magnetron Sputtering Thin Film preparation 2O 3(0001) substrate cleans: two kinds of substrates all need pass through acetone, alcohol and deionized water ultrasonic cleaning each 10 minutes; The Si substrate also need be put into 5% HF and soaked 2 ~ 3 minutes in addition, takes out and rinses well with deionized water; Use at last N 2Put into vacuum chamber after two kinds of samples are dried up;
2. magnetron sputtering equipment vacuumizes: after sample and target were all put into vacuum chamber, the plant machinery pump slightly was evacuated to below the 5Pa, then adopted molecular pump to carry out essence and vacuumized, and vacuum tightness is evacuated to 8.0 * 10 -4Pa;
3. after vacuum tightness reaches required high vacuum, be filled with purity and be 99.999% argon gas to air pressure 2Pa, allow the target build-up of luminance, then regulate argon flow amount to 10.0Sccm, operating air pressure modulation 0.5Pa, sputtering power 85 ~ 120W, target-substrate distance is 8 ~ 12cm, and sputtering time is 60 ~ 90min, after sputter is complete, apparatus cools 30min takes out ternary Fe-Si-Cr film sample.
Adopt the Fe of technique scheme preparation 3Cr 1Si xBe the noncrystalline membrane material, the growth velocity of film is about 5nm/min, prepared Fe 3Cr 1Si xThe band gap width of film can be modulated by the difference of Si content, so enlarge its use range.
At Si (100) and Al 2O 3(0001) prepares Fe on the substrate 3Cr 1Si x(x=8 ~ 18) film is with Cr element substitution β-FeSi 2A Fe element of/4th in the structure, the component proportions of the target alloy paster that adopts in the sputter procedure only has a kind of: Fe 3Cr 1, by changing the number of alloy slice, just can change Fe 3Cr 1Si xThe ratio of Si in the film, and then obtain having the noncrystalline membrane of different band gap widths.The method has processing condition and is easy to control, and the good uniformity of film is convenient to the advantages such as industrialization.Prepared film band gap is adjustable, and adhesion property is good, has a extensive future.
The invention has the beneficial effects as follows: this Fe-Cr-Si that modulates band gap width is that the ternary noncrystal membrane has following general formula: Fe 3Cr 1Si x, x is 8 ~ 18; Along with x is increased to 18 from 8, band gap width is increased to 0.65eV from 0, and membrane structure is always non-crystalline state.Fe 3Cr 1Si x(x=8 ~ 18) film is compared with common Dyadic transition metal silicide film and is had the following advantages: 1. Fe 3Cr 1Si xFilm is a kind of novel ternary semiconductor noncrystal membrane, can accomplish that the effect of Cr singly can not affect band gap width from 0 to 0.65eV internal modulation band gap width in a big way, and the amorphous formation ability that increases a constituent element film also can increase; 2. as long as change Fe in the combination sputtering target 3Cr 1The number of alloy slice just can be adjusted Fe easily 3Cr 1Si xThe ratio of Si in the film, and then obtain actual required different band gap widths; 3. prepared Fe 3Cr 1Si x(x=8 ~ 18) film is non-crystalline state, can guarantee that composition and performance are even, effectively avoids lattice mismatch and the heterogeneous problem such as mix in the crystalline film preparation.The narrow gap semiconductor devices such as suitable manufacturing near infrared detector.
Description of drawings
Fig. 1 is ternary noncrystal membrane Fe 3Cr 1Si 8TEM pattern picture and the selected area electron diffraction style in rete zone.
Fig. 2 is ternary noncrystal membrane Fe 3Cr 1Si 13.6TEM pattern picture and the selected area electron diffraction style in rete zone.
Fig. 3 is ternary noncrystal membrane Fe 3Cr 1Si 17.3TEM pattern picture and the selected area electron diffraction style in rete zone.
Fig. 4 is ternary noncrystal membrane Fe 3Cr 1Si 13.6(α T) 2-E relation curve.
Fig. 5 is ternary noncrystal membrane Fe 3Cr 1Si 17.3(α T) 2-E relation curve.
Among Fig. 1,2,3, by TEM result as can be known, the film base interface of the present invention's preparation is clear, rete is more smooth, continuous, and even thickness, and the selected area electron diffraction style in rete zone is significantly dispersed the ring except seeing, do not have other information, show that the film of preparation is non-crystalline state.
Among Fig. 4,5, X-coordinate is ENERGY E, and unit is eV, and ordinate zou is (α T) 2, arbitrary unit a.u.The ternary noncrystal membrane Fe of the present invention preparation as seen from the figure 3Cr 1Si 13.6And Fe 3Cr 1Si 17.3Band gap width be respectively 0.54eV, 0.60eV.
Embodiment
Be described in detail specific embodiments of the invention below in conjunction with technical scheme.
Embodiment 1: magnetically controlled sputter method prepares Fe 3Cr 1Si 8Film
(1) preparation alloy sputtering target, its step is as follows:
1. get the raw materials ready: take by weighing each constituent element value according to Fe and Cr atomic percent 3:1, the purity of stand-by Fe, Cr raw metal is more than 99.9%;
2. Fe 3Cr 1The melting of alloy pig: the compound of metal is placed in the water jacketed copper crucible of smelting furnace, adopts the method for vacuum arc melting under the protection of argon gas, to carry out melting, at first be evacuated to 10 -2Pa, then being filled with argon gas to air pressure is 0.03 ± 0.01MPa, the span of control of melting current density is 150 ± 10A/cm 2, after the fusing, continuing again 10 seconds of melting, outage allows alloy be cooled to room temperature with copper crucible, then with its upset, again places in the water jacketed copper crucible, carries out the melting second time; Aforementioned process melt back at least 3 times obtains the Fe of homogeneous chemical composition 3Cr 1Alloy pig;
3. Fe 3Cr 1The preparation of alloy bar: with Fe 3Cr 1Alloy pig places in the water jacketed copper crucible that is connected with negative pressure suction casting equipment, with above-mentioned vacuum arc melting method molten alloy, at first is evacuated to 10 under argon shield -2Pa, then being filled with argon gas to air pressure is 0.03 ± 0.01MPa, the used current density of melting is 150 ± 10A/cm 2, after the fusing, continuing again 10 seconds of melting, the negative pressure absorbing and casting device is opened in outage simultaneously, allows alloy melt be filled with in the cylindrical, copper model cavity, is cooled to room temperature, obtains the Fe that diameter is 10mm 3Cr 1Alloy bar;
4. the preparation of alloy paster: alloy bar is cut into the alloy small pieces that thickness is about 1.5mm with the low speed saw;
5. the preparation of alloy sputtering target: with conductive silver glue with 7 Fe 3Cr 1It is that (diameter is 75mm) makes the combined alloy sputtering target material on 99.999% the basic Si target that alloy slice sticks on the used purity of sputter.
(2) preparation Fe 3Cr 1Si 8The ternary noncrystal membrane, its step is as follows:
1. Si (100) and the Al of Magnetron Sputtering Thin Film preparation 2O 3(0001) substrate cleans; Two kinds of substrates all need pass through acetone, alcohol and deionized water ultrasonic cleaning each 10 minutes; The Si substrate also need be put into 5% HF and soaked 2～3 minutes in addition, takes out and rinses well with deionized water; Use at last N 2Put into vacuum chamber after two kinds of samples are dried up;
2. magnetron sputtering equipment extracting vacuum; After sample and target were all put into vacuum chamber, the plant machinery pump slightly was evacuated to below the 5Pa, then adopted molecular pump to carry out essence and vacuumized, and vacuum tightness is evacuated to 8.0 * 10 -4Pa;
3. after vacuum tightness reaches required high vacuum, be filled with argon gas (purity is 99.999%) to the air pressure 2Pa, allow the target build-up of luminance, then regulate argon flow amount to 10.0Sccm, operating air pressure modulation 0.5Pa, sputtering power 100W, target-substrate distance is about 10cm.Not also inartificial cooling of heating of substrate during sputter.Sputtering time is 60min, after sputter is complete, behind the apparatus cools 30min, takes out film sample.For preventing the sample oxidation, after the sample sputter is finished, do not take out as early as possible, take out again sample after half an hour with apparatus cools.
(3) analyze
Adopt the EPMA-1600 electron microprobe examination monitoring thin film composition of Japanese Shimadzu company, adopt German Brooker D8 discover film X-ray diffractometer (XRD), Philips Technai G 2The type transmission electron microscope carries out microstructure analysis to film.Band gap width is analyzed by UV3600 type ultraviolet-visible-near infrared spectrometer.
The content of Fe, Cr, three kinds of elements of Si is followed successively by 24.9at.%, 8.5at.%, 66.6at.% in the EPMA analysed film.The atomic ratio of Fe, Cr is 3:1, so write empirical formula as Fe 3Cr 1Si 8XRD and TEM detected result show at Fe 3Cr 1Si 8Do not find crystal information in the sample, what preparation was described is the amorphous film.The thickness of TEM image measurement film is 310nm, does not observe obvious absorption when band gap width is measured, so this moment, band gap width was 0eV.
Embodiment 2: magnetically controlled sputter method prepares Fe 3Cr 1Si 13.6Film
Preparation process is identical with embodiment 1, only adjusts the alloy slice number of preparation combined alloy sputtering target material: by 5 Fe 3Cr 1Alloy slice sticks on the used basic Si target of sputter and makes.The content of Fe, Cr, three kinds of elements of Si is followed successively by 16.9at.%, 5.7at.%, 77.4at.% in the EPMA analysed film.The atomic ratio of Fe, Cr is 3:1, so write empirical formula as Fe 3Cr 1Si 13.6XRD and TEM detected result show at Fe 3Cr 1Si 13.6Do not find crystal information in the sample, what preparation was described is the amorphous film.The thickness of TEM image measurement film is 315nm, and band gap width is measured as 0.54eV.
Embodiment 3: magnetically controlled sputter method prepares Fe 3Cr 1Si 17.3Film
Preparation process is identical with embodiment 1, only adjusts the alloy slice number of preparation combined alloy sputtering target material: by 4 Fe 3Cr 1Alloy slice sticks on the used basic Si target of sputter and makes.The content of Fe, Cr, three kinds of elements of Si is followed successively by 14.1 at.%, 4.7at.%, 81.2at.% in the EPMA analysed film.The atomic ratio of Fe, Cr is 3:1, so write empirical formula as Fe 3Cr 1Si 17.3XRD and TEM detected result show at Fe 3Cr 1Si 17.3Do not find crystal information in the sample, what preparation was described is the amorphous film.The thickness of TEM image measurement film is 323nm, and band gap width is measured as 0.60eV.

Claims (2)

1. the Fe-Cr-Si that can modulate band gap width is the ternary noncrystal membrane, it is characterized in that: have following general formula: Fe 3Cr 1Si x, x is 8 ~ 18; Along with x is increased to 18 from 8, the band gap width of this Amorphous Films is increased to 0.65eV from 0, and membrane structure is always non-crystalline state.
2. the Fe-Si-Cr that the modulates band gap width according to claim 1 preparation method that is the ternary noncrystal membrane is characterized in that: adopt the following step:
(1) preparation alloy sputtering target, its step is as follows:
1. get the raw materials ready: take by weighing each constituent element value according to Fe and Cr atomic percent 3:1, the purity of stand-by Fe, Cr raw metal is more than 99. 9%;
2. Fe 3Cr 1The melting of alloy pig: the compound of metal is placed in the water jacketed copper crucible of smelting furnace, adopts the method for vacuum arc melting under the protection of argon gas, to carry out melting, at first be evacuated to 10 -2Pa, then being filled with argon gas to air pressure is 0.03 ± 0.01MPa, the span of control of melting current density is 150 ± 10A/cm 2, after the fusing, continuing again 10 seconds of melting, outage allows alloy be cooled to room temperature with copper crucible, then with its upset, again places in the water jacketed copper crucible, carries out the melting second time; Aforementioned process melt back at least 3 times obtains the Fe of homogeneous chemical composition 3Cr 1Alloy pig;
3. Fe 3Cr 1The preparation of alloy bar: with Fe 3Cr 1Alloy pig places in the water jacketed copper crucible that is connected with negative pressure suction casting equipment, with above-mentioned vacuum arc melting method molten alloy, at first is evacuated to 10 under argon shield -2Pa, then being filled with argon gas to air pressure is 0.03 ± 0.01MPa, the used current density of melting is 150 ± 10A/cm 2, after the fusing, continuing again 10 seconds of melting, the negative pressure absorbing and casting device is opened in outage simultaneously, allows alloy melt be filled with in the cylindrical, copper model cavity, is cooled to room temperature, obtains requiring the Fe of specification 3Cr 1Alloy bar;
4. the preparation of alloy paster: the alloy small pieces that alloy bar are cut into desired thickness with the low speed saw;
5. the preparation of alloy sputtering target: with conductive silver glue with Fe 3Cr 1It is on 99.999% the basic Si target, perhaps with Fe that alloy slice sticks on the used purity of sputter 3Cr 1It is to make the combined alloy sputtering target material on the 99.999% basic Si target that alloy slice directly is mounted to porose purity;
(2) preparation Fe-Si-Cr is the ternary noncrystal membrane, and its step is as follows:
1. Si (100) and the Al of Magnetron Sputtering Thin Film preparation 2O 3(0001) substrate cleans: two kinds of substrates all need pass through acetone, alcohol and deionized water ultrasonic cleaning each 10 minutes; The Si substrate also need be put into 5% HF and soaked 2 ~ 3 minutes in addition, takes out and rinses well with deionized water; Use at last N 2Put into vacuum chamber after two kinds of samples are dried up;
2. magnetron sputtering equipment vacuumizes: after sample and target were all put into vacuum chamber, the plant machinery pump slightly was evacuated to below the 5Pa, then adopted molecular pump to carry out essence and vacuumized, and vacuum tightness is evacuated to 8.0 * 10 -4Pa;
3. after vacuum tightness reaches required high vacuum, be filled with purity and be 99.999% argon gas to air pressure 2Pa, allow the target build-up of luminance, then regulate argon flow amount to 10.0Sccm, operating air pressure modulation 0.5Pa, sputtering power 85 ~ 120W, target-substrate distance is 8 ~ 12cm, and sputtering time is 60 ~ 90min, after sputter is complete, apparatus cools 30min takes out ternary Fe-Cr-Si film sample.
CN201310016602.1A 2013-01-17 2013-01-17 Fe-Cr-Si ternary amorphous thin film capable of modulating band gap width and preparation method thereof Expired - Fee Related CN103074553B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103572353A (en) * 2013-10-29 2014-02-12 芜湖普威技研有限公司 Electrophoresis protective device for automobile rear axle end
CN103643305A (en) * 2013-12-04 2014-03-19 北京华进创威电子有限公司 Preparation method of TaC crucible for high-temperature gas phase method crystal growth

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CN102808150A (en) * 2012-09-12 2012-12-05 大连理工大学 Cu-Ni-Nb ternary alloy film with low resistivity and high chemical inertia and preparation process thereof

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CN102808150A (en) * 2012-09-12 2012-12-05 大连理工大学 Cu-Ni-Nb ternary alloy film with low resistivity and high chemical inertia and preparation process thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103572353A (en) * 2013-10-29 2014-02-12 芜湖普威技研有限公司 Electrophoresis protective device for automobile rear axle end
CN103643305A (en) * 2013-12-04 2014-03-19 北京华进创威电子有限公司 Preparation method of TaC crucible for high-temperature gas phase method crystal growth

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